EPA Method 552

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EPA Method 552:
DETERMINATION OF HALOACETIC ACIDS IN DRINKING WATER BY LIQUIDLIQUID EXTRACTION, DERIVATIZATION, AND GAS CHROMATOGRAPHY WITH ELECTRON CAPTURE DETECTION

Summary:
A 100 mL volume of sample is adjusted to pH 11.5 and extracted with methyltert- butyl ether (MTBE) to remove neutral and basic organic compounds. The aqueous sample is then acidified to pH 0.5 and the acids are extracted into MTBE. After the extract is dried and concentrated, the acids are converted to their methyl esters with diazomethane (DAM). Excess DAM is removed and the methyl esters are determined by capillary GC using an electron capture detector (ECD). An alternative microextraction procedure is also offered in which a 30 mL sample is extracted without cleanup with a single 3 mL aliquot of MTBE for direct analysis by GC-ECD after methylation. Samples containing high concentrations of haloacetic acids and other disinfection byproducts, or other potentially interfering organic compounds, may require the sample cleanup.

Scope:
This is a gas chromatographic (GC) method1-4,11 applicable to the determination of the listed halogenated acetic acids in drinking water, ground water, raw water and any intermediate treatment stage. In addition, the chlorinated phenols listed may be analyzed by this method.

Report Number:
600/4-90-020